CN106564871B - A kind of crystal whisker-shaped thin film bio carbon material and preparation method thereof - Google Patents
A kind of crystal whisker-shaped thin film bio carbon material and preparation method thereof Download PDFInfo
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
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Abstract
The invention discloses a kind of crystal whisker-shaped thin film bio carbon materials and preparation method thereof, are template using calcium carbonate crystal whisker, load poly-dopamine film, form CaCO3@PDA composite material generates intermediate product CaO@W-HFGB through high temperature cabonization, is soaked in water to form Ca (OH)2Crystal whisker-shaped thin film bio carbon material is made through secondary carbonization reaming [email protected] present invention has carried out efficient utilization to environmentally protective template calcium carbonate crystal whisker, while having carried out dual reaming from physics and chemically to W-HFGB as expanding agent, avoids and introduces new expanding agent；Furthermore advantage of the invention is that：The various features such as preparation cost is low, process is environmentally protective, product structure is novel have great application potential in industrialization.
Description
Technical field
The invention belongs to material chemistry technical fields, and in particular to a kind of crystal whisker-shaped thin film bio carbon material and its preparation side
Method.
Background technique
Extensive use of the porous carbon materials of special appearance in the fields such as absorption, separation and catalysis in recent years, causes
More and more attention of people.Wherein preparing the common method of porous carbon materials has hard template method, soft template method, activation method.
Activation method is that activator under high temperature environment performs etching carbon matrix precursor, generates a large amount of nanoscale cracks or smaller mesoporous.Often
The activating reagent seen has KOH, NaOH, ZnCl2、H3PO4Deng.
Dopamine (dopamine, 3,4- dihydroxy propyl benzene amine), is the important composition ingredient of marine mussel secretion, has
Oxidation self-polymeric reaction occurs easily under wet condition for the features such as nontoxic, good biocompatibility, strongly adherent, in surface of solids shape
At poly-dopamine (PDA, polydopamine) film.Poly-dopamine film can prepare the presoma of porous carbon materials, in height
It is carbonized under the conditions of temperature, forms the carbon material of dense non-porous, under the further etching carbonization of expanding agent, generate porous carbon materials.
It prepares in the porous carbon materials of special appearance, generally there are the removal of template difficulty and expanding agent is with high costs etc. asks
Topic.Calcium carbonate is a kind of environmentally friendly inorganic raw material, has many advantages, such as cheap, nontoxic, to have removed.It can benefit
With the calcium carbonate product of different-shape, it is applied to as template in the preparation of the porous carbon materials of special appearance.
The disclosure of background above technology contents is only used for auxiliary and understands design and technical solution of the invention, not necessarily
The prior art for belonging to present patent application, no tangible proof show above content present patent application the applying date
In disclosed situation, above-mentioned background technique should not be taken to the novelty and creativeness of evaluation the application.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of crystal whisker-shaped thin film bio carbon materials and preparation method thereof, with solution
The problems such as certainly existing template difficulty removal, expanding agent is with high costs.The present invention to environmentally protective template calcium carbonate crystal whisker into
It has gone efficient utilization, while having carried out dual reaming from physics and chemically to W-HFGB as expanding agent, it is new to avoid introducing
Expanding agent；Furthermore advantage of the invention is that：The various features such as preparation cost is low, process is environmentally protective, product structure is novel,
There is great application potential in industrialization.
In order to solve the above technical problems, the present invention uses following technical scheme：
For this purpose, the present invention proposes a kind of crystal whisker-shaped thin film bio carbon material, being is template, load using calcium carbonate crystal whisker
Poly-dopamine film forms CaCO3@PDA composite material generates intermediate product CaO@W-HFGB through high temperature cabonization, is soaked in water
It is formed Ca (OH)2Crystal whisker-shaped thin film bio carbon material is made through secondary carbonization reaming in@W-HFGB.
The present invention also provides a kind of preparation methods of crystal whisker-shaped thin film bio carbon material, include the following steps：
(1) synthesis of calcium carbonate crystal whisker
Digestion reaction occurs at 80 DEG C by raw material and tap water of calcium oxide, matches after ageing, filtering, removal step
Ca (OH) processed2Suspension is added in the circulation feed liquid kettle into supergravity reactor；It controls Ca (OH)2Suspension total amount of feeding,
In CO2Gas flow is 50Lh-1, fluid flow 530Lh-1, chemical additives additional amount is 7gL-1, carburizing temperature
It is 60~85 DEG C, revolving bed revolving speed is 1000~1600rmin-1Preparation process condition under, Ca (OH)2Suspension and CO2Gas
Body generates calcium carbonate crystal whisker in the raw carburizing reagent of the inscribed triggering of rotary packed bed；Reaction rear slurry is filtered, uses deionization
Water washs repeatedly, 80 DEG C of vacuum drying 5h, and calcium carbonate crystal whisker product is made；
(2)Ca(OH)2The preparation of@W-HFGB composite material
Compound concentration is 4~7gL respectively-1Dopamine saline solution 100mL, concentration 8gL-1Calcium carbonate crystal whisker water
Solution 50ml, and the alkaline solution prepared by 0.75mL ammonium hydroxide, 40mL ethyl alcohol, 90mL deionized water, three kinds of different solutions point
It Mi Feng not stir evenly；Configured calcium carbonate aqueous solution is added into DOPA amine salt aqueous solution, in bath temperature 15~25
DEG C, 150~300rmin of speed of agitator-1Under conditions of, react 0.5h；Prepared alkaline solution is added to above-mentioned DOPA
In amine salt mixed solution, reaction temperature is remained unchanged with revolving speed, reacts 20h；Reaction rear slurry is filtered, uses deionized water
CaCO is made in washing, 80 DEG C of vacuum drying 5h3@PDA composite material；Weigh CaCO3@PDA sample is placed in tube furnace, in nitrogen
Protection under, carry out high temperature cabonization, obtain CaO@W-HFGB；It is put into CaO@W-HFGB in magnetic boat, deionized water is added to impregnate, it is quiet
It sets, generates Ca (OH)2@W-HFGB is dried in vacuo it at 70 DEG C, obtains Ca (OH)2@W-HFGB composite powder；
(3) preparation of crystal whisker-shaped thin film bio carbon material
Weigh Ca (OH)2@W-HFGB sample is placed in tube furnace, under the protection of nitrogen, carries out secondary high-temperature carbonization,
Middle Ca (OH)2Reaming is performed etching to W-HFGB, is washed with deionized water to neutrality after reaction, filter cake is finally put into 80
DEG C vacuum oven in dry 5h, obtain crystal whisker-shaped thin film bio carbon material.
Further, calcium oxide described in step (1) is technical grade.
Further, Ca (OH) described in step (1)2The concentration of suspension is 60~90gL-1。
Further, the Ca (OH) of control described in step (1)2Suspension total amount of feeding is 2.8L.
Further, chemical additives described in step (1) are phosphoric acid.
Further, the weight ratio of DOPA amine salt described in step (2) and calcium carbonate crystal whisker is：1.00~1.75:
1.00。
Further, the ratio of CaO@W-HFGB described in step (2) and deionized water is：0.2~0.8g:10mL.
Further, time of repose described in step (2) is 6h.
Further, step (2) is identical with high temperature cabonization program described in (3), includes the following steps：
(a) temperature-rise period：With 5~15 DEG C of min-1Speed sample is risen to 700~900 DEG C from room temperature；
(b) thermostatic process：Sample is in 700~900 DEG C of 1~3h of holding；
(c) temperature-fall period：Sample is from 700~900 DEG C of cooled to room temperatures.
Compared with prior art, the present invention having the advantages that：
(1) present invention resolves into calcium oxide and carbon dioxide after high temperature cabonization, uses water using calcium carbonate crystal whisker as template
Calcium oxide can be removed, solves the problems, such as the removal of later period template difficulty；
(2) calcium carbonate crystal whisker used in the present invention decomposes the CO of release in first time carbonisation2With efficient
Reaming effect；
(3) calcium carbonate crystal whisker pyrolytic of the invention, the Ca formed after soaking in water (OH)2, in secondary carbonisation
In can be used as expanding agent, realize the efficient utilization to calcium carbonate crystal whisker.
Detailed description of the invention
Fig. 1 is one calcium carbonate crystal whisker of the embodiment of the present invention and SEM and the TEM figure of W-HFGB；
Fig. 2 is the XRD diagram of one calcium carbonate crystal whisker of the embodiment of the present invention, CaO@W-HFGB and W-HFGB；
Fig. 3 is one calcium carbonate crystal whisker of the embodiment of the present invention, CaCO3The TG of@PDA schemes；
Fig. 4 is the N of one W-HFGB of the embodiment of the present invention2Adsorption-desorption figure.
Specific embodiment
With reference to embodiment and compares attached drawing invention is further described in detail.It is emphasized that
Following the description is only exemplary, the range and its application being not intended to be limiting of the invention.
Embodiment 1
A kind of preparation method of crystal whisker-shaped thin film bio carbon material, includes the following steps：
(1) synthesis of calcium carbonate crystal whisker
With technical grade calcium oxide (quick lime) for raw material and tap water, digestion reaction occurs at 80 DEG C, by ageing, mistake
Filter, removal of impurities and etc. after be configured to concentration be 80gL-1Ca (OH)2The circulation into supergravity reactor is added in suspension
In feed liquid kettle；The Ca (OH) of control2Suspension total amount of feeding is 2.8L, in CO2Gas flow is 50Lh-1, fluid flow is
530L·h-1, chemical additives phosphoric acid additional amount is 7gL-1, carburizing temperature is 70 DEG C, and revolving bed revolving speed is 1400rmin-1
Preparation process condition under, Ca (OH)2Suspension and CO2Gas generates carbonic acid in the raw carburizing reagent of the inscribed triggering of rotary packed bed
Calcium pyroborate；
(2)Ca(OH)2The preparation of@W-HFGB composite material
Compound concentration is 5gL-1DOPA amine salt (DA) aqueous solution 100mL, concentration 8gL-1Calcium carbonate crystal whisker aqueous solution
50ml, i.e. weight ratio are 1.25DA/1.0CaCO3DOPA amine salt and calcium carbonate crystal whisker, and by 0.75mL ammonium hydroxide, 40mL
Ethyl alcohol, the alkaline solution that 90mL deionized water is prepared, three kinds of different solutions seal respectively to stir evenly；By configured calcium carbonate
Aqueous solution is added into DOPA amine salt aqueous solution, is 20 DEG C in bath temperature, speed of agitator 200rmin-1Under conditions of, instead
Answer 0.5h；Prepared alkaline solution is added in above-mentioned dopamine mixed salt solution, reaction temperature is remained unchanged with revolving speed,
20h is reacted, CaCO is made3@PDA composite material；
(3) preparation of crystal whisker-shaped thin film bio carbon material
Weigh the CaCO of certain mass3@PDA sample is placed in tube furnace, under the protection of nitrogen, carries out high temperature cabonization,
Carbonization Conditions are：With 5 DEG C of min-1Speed by CaCO3@PDA sample rises to 700 DEG C, constant temperature 1h, then natural cooling from room temperature
To room temperature, CaO@W-HFGB is obtained.It is put into 0.4g CaO@W-HFGB in magnetic boat, 10mL ionized water is added to impregnate, stands 6h,
It generates Ca (OH)2@W-HFGB is dried in vacuo it at 70 DEG C, obtains Ca (OH)2@W-HFGB powder；Weigh certain mass
Ca (OH)2@W-HFGB sample is placed in tube furnace, under the protection of nitrogen, carries out secondary high-temperature carbonization, carbodiimide procedure is not
Become, wherein Ca (OH)2Reaming is performed etching to W-HFGB, is washed with deionized water to neutrality after reaction, finally obtains carbon
Material W-HFGB-1.
Embodiment 2
In addition to following variations, remaining is the same as embodiment 1.
Compound concentration is 6gL-1DOPA amine salt (DA) aqueous solution 100mL, concentration 8gL-1Calcium carbonate crystal whisker aqueous solution
50ml, i.e. weight ratio are 1.50DA/1.0CaCO3DOPA amine salt and calcium carbonate crystal whisker, and by 0.75mL ammonium hydroxide, 40mL
Ethyl alcohol, the alkaline solution that 90mL deionized water is prepared, three kinds of different solutions seal respectively to stir evenly；By configured calcium carbonate
Aqueous solution is added into DOPA amine salt aqueous solution, at 25 DEG C of bath temperature, speed of agitator 250rmin-1Under conditions of, reaction
0.5h；Prepared alkaline solution is added in above-mentioned dopamine mixed salt solution, reaction temperature is remained unchanged with revolving speed, instead
Answer 20h that intermediate product CaCO is made3@PDA；
Weigh the CaCO of certain mass3@PDA sample is placed in tube furnace, under the protection of nitrogen, carries out high temperature cabonization,
Carbonization Conditions are：With 10 DEG C of min-1Speed by CaCO3@PDA sample rises to 800 DEG C, constant temperature 2h, then natural cooling from room temperature
To room temperature；Obtain intermediate product CaO@W-HFGB；It is put into 0.6g CaO@W-HFGB in magnetic boat, 10mL ionized water is added to impregnate,
6h is stood, is generated Ca (OH)2@W-HFGB is dried in vacuo it at 70 DEG C, obtains Ca (OH)2@W-HFGB powder.Keep carbon
Change the constant secondary carbonization of progress of program, is washed with deionized water to neutrality after reaction, it is final to obtain carbon material W-HFGB-2.
Embodiment 3
In addition to following variations, remaining is the same as embodiment 1.
Compound concentration is 7gL-1DOPA amine salt (DA) aqueous solution 100mL, concentration 8gL-1Calcium carbonate crystal whisker aqueous solution
50ml, i.e. weight ratio are 1.75DA/1.0CaCO3DOPA amine salt and calcium carbonate crystal whisker, and by 0.75mL ammonium hydroxide, 40mL
Ethyl alcohol, the alkaline solution that 90mL deionized water is prepared, three kinds of different solutions seal respectively to stir evenly；By configured calcium carbonate
Aqueous solution is added into DOPA amine salt aqueous solution, at 15 DEG C of bath temperature, speed of agitator 300rmin-1Under conditions of, reaction
0.5h；Prepared alkaline solution is added in above-mentioned dopamine mixed salt solution, reaction temperature is remained unchanged with revolving speed, instead
Answer 20h that intermediate product CaCO is made3@PDA；
Weigh the CaCO of certain mass3@PDA sample is placed in tube furnace, under the protection of nitrogen, carries out high temperature cabonization,
Carbonization Conditions are：With 15 DEG C of min-1Speed by CaCO3@PDA sample rises to 900 DEG C, constant temperature 3h, then natural cooling from room temperature
To room temperature；Obtain intermediate product CaO@W-HFGB；It is put into 0.8g CaO@W-HFGB in magnetic boat, 10mL ionized water is added to impregnate,
6h is stood, is generated Ca (OH)2@W-HFGB is dried in vacuo it at 70 DEG C, obtains Ca (OH)2@W-HFGB powder；Keep carbon
Change the constant secondary carbonization of progress of program, is washed with deionized water to neutrality after reaction, it is final to obtain carbon material W-HFGB-3.
Instance analysis
As shown in Figure 1, W-HFGB porous carbon materials prepared by the present invention, the appearance structure with whisker film-form, show
Template calcium carbonate has resolved into calcium oxide completely and has been washed with water removal, and pattern does not collapse after wash water.Wherein SEM chart is bright
The minor axis of t calcium carbonate crystal whisker is 140~180nm, and draw ratio is 17~20.
As shown in Fig. 2, it is aragonitic that the present invention, which prepares calcium carbonate crystal whisker, and the XRD spectrum of intermediate product CaO@W-HFGB
Characteristic peak without calcium carbonate aragonitic, shows CaCO3Calcium carbonate in@PDA resolves into calcium oxide completely.Wherein W-HFGB
XRD diagram, 26 ° and 44 ° it is upper there is graphitization characteristic peak, (002) and (100) crystal face shows W-HFGB with part graphite
Change structure.
As shown in figure 3, calcium carbonate crystal whisker prepared by the present invention and CaCO3@PDA decomposition temperature, respectively 586 DEG C and 673
DEG C, wherein CaCO3@PDA weight-loss ratio under conditions of greenhouse rises to 900 DEG C is about 57%.
As shown in figure 4, the N of W-HFGB prepared by the present invention2Adsorption/desorption figure, and its thus obtain the pore structure of material
As shown in table 1.Know that W-HFGB has high-specific surface area and big micro-diplopore structure, BET are respectively with Langmuir specific surface area
707.4m2·g-1, 843.9m2·g-1, wherein micropore ratio is 38.38%.
The pore structure parameter of 1 W-HFGB of table
It would be recognized by those skilled in the art that above description make numerous accommodations be it is possible, so embodiment and attached
Figure is intended merely to describe one or more particular implementations.
It is counted as example embodiment of the invention although having been described and describing, it will be apparent to those skilled in the art that
It can be variously modified and is replaced, without departing from spirit of the invention.Furthermore it is possible to make many modifications with will be special
Condition of pledging love is fitted to religious doctrine of the invention, without departing from invention described herein central concept.So the present invention is unrestricted
In specific embodiment disclosed herein, but the present invention may further include belonging to all embodiments of the scope of the invention and its being equal
Object.
Claims (9)
1. a kind of preparation method of crystal whisker-shaped thin film bio carbon material, which is characterized in that the crystal whisker-shaped thin film bio carbon material
Being is template using calcium carbonate crystal whisker, and load poly-dopamine film forms CaCO3@PDA composite material, through pyrocarbon metaplasia
At intermediate product CaO@W-HFGB, it is soaked in water to form Ca (OH)2@W-HFGB is made through secondary carbonization reaming；
The preparation method of the crystal whisker-shaped thin film bio carbon material, includes the following steps：
(1) synthesis of calcium carbonate crystal whisker
Digestion reaction occurs at 80 DEG C by raw material and tap water of calcium oxide, prepares Ca after ageing, filtering, removal step
(OH)2Suspension is added in the circulation feed liquid kettle into supergravity reactor；It controls Ca (OH)2Suspension total amount of feeding, in CO2
Gas flow is 50Lh-1, fluid flow 530Lh-1, chemical additives additional amount is 7gL-1, carburizing temperature be 60~
85 DEG C, revolving bed revolving speed is 1000~1600rmin-1Preparation process condition under, Ca (OH)2Suspension and CO2Gas is revolving
Turn the raw carburizing reagent of the inscribed triggering of packed bed and generates calcium carbonate crystal whisker；Will reaction rear slurry filtered, with deionized water repeatedly
Calcium carbonate crystal whisker product is made in washing, 80 DEG C of vacuum drying 5h；
(2)Ca(OH)2The preparation of@W-HFGB composite material
Compound concentration is 4~7gL respectively-1Dopamine saline solution 100mL, concentration 8gL-1Calcium carbonate crystal whisker aqueous solution
50ml, and the alkaline solution prepared by 0.75mL ammonium hydroxide, 40mL ethyl alcohol, 90mL deionized water, three kinds of different solutions difference are close
Envelope stirs evenly；Configured calcium carbonate aqueous solution is added into DOPA amine salt aqueous solution, at 15~25 DEG C of bath temperature, is stirred
Mix 150~300rmin of revolving speed-1Under conditions of, react 0.5h；Prepared alkaline solution is added to above-mentioned DOPA amine salt to mix
It closes in solution, reaction temperature is remained unchanged with revolving speed, reacts 20h；Reaction rear slurry is filtered, is washed with deionized,
CaCO is made in 80 DEG C of vacuum drying 5h3@PDA composite material；Weigh CaCO3@PDA sample is placed in tube furnace, in the guarantor of nitrogen
Under shield, high temperature cabonization is carried out, obtains CaO@W-HFGB；It is put into CaO@W-HFGB in magnetic boat, deionized water is added to impregnate, stands,
It generates Ca (OH)2@W-HFGB is dried in vacuo it at 70 DEG C, obtains Ca (OH)2@W-HFGB composite powder；
(3) preparation of crystal whisker-shaped thin film bio carbon material
Weigh Ca (OH)2@W-HFGB sample is placed in tube furnace, under the protection of nitrogen, carries out secondary high-temperature carbonization, wherein Ca
(OH)2Reaming is performed etching to W-HFGB, is washed with deionized water to neutrality after reaction, filter cake is finally put into 80 DEG C
Dry 5h, obtains crystal whisker-shaped thin film bio carbon material in vacuum oven.
2. the preparation method of crystal whisker-shaped thin film bio carbon material according to claim 1, which is characterized in that in step (1)
The calcium oxide is technical grade.
3. the preparation method of crystal whisker-shaped thin film bio carbon material according to claim 2, which is characterized in that in step (1)
The Ca (OH)2The concentration of suspension is 60~90gL-1。
4. the preparation method of crystal whisker-shaped thin film bio carbon material according to claim 1, which is characterized in that in step (1)
The Ca (OH) of the control2Suspension total amount of feeding is 2.8L.
5. the preparation method of crystal whisker-shaped thin film bio carbon material according to claim 1, which is characterized in that in step (1)
The chemical additives are phosphoric acid.
6. the preparation method of crystal whisker-shaped thin film bio carbon material according to claim 1, it is characterised in that：In step (2)
The weight ratio of the DOPA amine salt and calcium carbonate crystal whisker is：1.00~1.75:1.00.
7. the preparation method of crystal whisker-shaped thin film bio carbon material according to claim 1, it is characterised in that：In step (2)
The ratio of the CaO@W-HFGB and deionized water is：0.2~0.8g:10mL.
8. the preparation method of crystal whisker-shaped thin film bio carbon material according to claim 1, it is characterised in that：In step (2)
The time of repose is 6h.
9. the preparation method of crystal whisker-shaped thin film bio carbon material according to claim 1, it is characterised in that：Step (2) and
(3) high temperature cabonization program described in is identical, includes the following steps：
(a) temperature-rise period：With 5~15 DEG C of min-1Speed sample is risen to 700~900 DEG C from room temperature；
(b) thermostatic process：Sample is in 700~900 DEG C of 1~3h of holding；
(c) temperature-fall period：Sample is from 700~900 DEG C of cooled to room temperatures.
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